Method for producing molecular compound

Abstract

A method for producing a molecular compound which comprises mixing and kneading a solid host compound and a solid or liquid guest compound by using a kneader and optionally followed by extruding and granulating, wherein the method further comprises one or more of the steps of holding the product at a temperature which is 50° C. or higher and not higher than the emission temperature for the guest compound, washing the formed molecular compound with a solvent capable of dissolving the guest compound, pulverizing in advance the solid host compound, and adding a poor solvent such as water prior to mixing and kneading. The method allows the production of a molecular compound having improved stability.

1. A method for producing a clathrate having improved stability which comprises mixing and/or kneading a solid tetrakisphenol host compound with a solid or liquid cyclic aliphatic amine guest compound, and comprising at least one of the following steps: (a) pulverizing the solid host compound by a jet stream prior to mixing and/or kneading; or (b) adding a poor solvent in an amount of between 200 ml and 1000 ml to a mole of the solid tetrakisphenol host compound prior to mixing and/or kneading, the poor solvent being a solvent that dissolves 1 g/100 ml or less of the solid tetrakisphenol host compound and the solid or liquid cyclic aliphatic amine guest compound at room temperature. 
     
     
       2. A method according to  claim 1  in which the solid host compound is pulverized to an average particle size of 1.6 μm or smaller in Step (a). 
     
     
       3. A method according to  claim 1  in which the solid host compound is pulverized to a particle size of 4.0 μm or smaller in Step (a). 
     
     
       4. A method according to  claim 1 , in which 80% by weight or more of the solid host compound is pulverized to 2.0 μm or smaller in particle size in Step (a). 
     
     
       5. A method according to  claim 1 , in which the poor solvent is added at an amount of 20 to 200% by weight to the total weight of the solid host compound and the solid or liquid guest compound prior to mixing and/or kneading in Step (b). 
     
     
       6. A method according to  claim 1 , in which the poor solvent is added, and the host compound is mixed and/or kneaded with the guest compound while heating so that the content of the solvent becomes 1% by weight or below in Step (b). 
     
     
       7. A method according to  claim 1 , in which the poor solvent is added to the host and guest compounds to mix and/or knead, followed by drying the product so that the content of the solvent is 1% by weight or less in Step (b). 
     
     
       8. A method according to  claim 1 , in which the poor solvent used in Step (b) is water. 
     
     
       9. A method according to  claim 1 , in which the solid host compound is mixed with a required amount of the solid guest compound or with a necessary amount of the liquid guest compound all at once. 
     
     
       10. A method for producing a clathrate comprising: pulverizing a solid tetrakisphenol host compound an average particle size of 1.6 μm or smaller; and dispersing the pulverized solid tetrakisphenol host compound and a solid or liquid cyclic aliphatic amine guest compound in a poor solvent, the solid tetrakisphenol host compound being from 10 to 50% by weight in concentration, and the poor solvent being a solvent that dissolves 1 g/100 ml or less of the solid tetrakisphenol host compound and the solid or liquid cyclic aliphatic amine guest compound at room temperature. 
     
     
       11. A method for producing a clathrate comprising: pulverizing a solid tetrakisphenol host compound to a particle size of 4.0 μm or smaller; and dispersing the pulverized solid tetrakisphenol host compound and a solid or liquid cyclic aliphatic amine guest compound in a poor solvent, the solid tetrakisphenol host compound being from 10 to 50% by weight in concentration, and the poor solvent being a solvent that dissolves 1 g/100 ml or less of the solid tetrakisphenol host compound and the solid or liquid cyclic aliphatic amine guest compound at room temperature. 
     
     
       12. A method for producing a clathrate comprising: pulverizing 80% by weight or more of a solid tetrakisphenol host compound to 2.0 μm or smaller in particle size; and dispersing the pulverized host tetrakisphenol compound and a solid or liquid cyclic aliphatic amine guest compound in a poor solvent, the solid tetrakisphenol host compound being from 10 to 50% by weight in concentration, the poor solvent being a solvent that dissolves 1 g/100 ml or less of the solid tetrakisphenol host compound and the solid or liquid cyclic aliphatic amine guest compound at room temperature. 
     
     
       13. A method according to one of  claims 10  to  12  in which the solid host compound is pulverized by a jet stream. 
     
     
       14. A method according to one of  claims 10  to  12 , in which the poor solvent is water. 
     
     
       15. A method according to one of  claims 1 ,  10 ,  11  or  12 , in which the solid tetrakisphenol host compound is 1,1,2,2-tetrakis(4-hydroxyphenyl)ethane.